EP3794647B1 - Method for producing light emitting diodes (leds) by one step film lamination - Google Patents
Method for producing light emitting diodes (leds) by one step film lamination Download PDFInfo
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- EP3794647B1 EP3794647B1 EP18918870.9A EP18918870A EP3794647B1 EP 3794647 B1 EP3794647 B1 EP 3794647B1 EP 18918870 A EP18918870 A EP 18918870A EP 3794647 B1 EP3794647 B1 EP 3794647B1
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- EP
- European Patent Office
- Prior art keywords
- phosphor
- silicone binder
- catalyst
- leds
- colored
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- 238000003475 lamination Methods 0.000 title claims description 29
- 238000004519 manufacturing process Methods 0.000 title claims description 15
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 claims description 166
- 239000011230 binding agent Substances 0.000 claims description 67
- 229920001296 polysiloxane Polymers 0.000 claims description 67
- 239000003054 catalyst Substances 0.000 claims description 48
- 239000000203 mixture Substances 0.000 claims description 44
- 239000003795 chemical substances by application Substances 0.000 claims description 27
- 238000000034 method Methods 0.000 claims description 19
- 238000001035 drying Methods 0.000 claims description 17
- 230000009977 dual effect Effects 0.000 claims description 16
- 239000006185 dispersion Substances 0.000 claims description 9
- 150000007514 bases Chemical group 0.000 claims description 3
- 238000010030 laminating Methods 0.000 claims description 3
- -1 aluminum alkoxides Chemical class 0.000 description 26
- 238000000518 rheometry Methods 0.000 description 23
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 description 15
- 239000011268 mixed slurry Substances 0.000 description 12
- 229910052719 titanium Inorganic materials 0.000 description 12
- 239000010936 titanium Substances 0.000 description 12
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 11
- 238000001723 curing Methods 0.000 description 10
- 238000009472 formulation Methods 0.000 description 10
- 238000006459 hydrosilylation reaction Methods 0.000 description 10
- 238000002360 preparation method Methods 0.000 description 9
- 238000002156 mixing Methods 0.000 description 8
- 125000005375 organosiloxane group Chemical group 0.000 description 8
- 229910000831 Steel Inorganic materials 0.000 description 7
- 239000003960 organic solvent Substances 0.000 description 7
- 239000010959 steel Substances 0.000 description 7
- 239000011248 coating agent Substances 0.000 description 6
- 238000000576 coating method Methods 0.000 description 6
- 239000000463 material Substances 0.000 description 6
- 238000010998 test method Methods 0.000 description 6
- 229910052726 zirconium Inorganic materials 0.000 description 6
- 239000008393 encapsulating agent Substances 0.000 description 5
- 238000002203 pretreatment Methods 0.000 description 5
- WADSJYLPJPTMLN-UHFFFAOYSA-N 3-(cycloundecen-1-yl)-1,2-diazacycloundec-2-ene Chemical compound C1CCCCCCCCC=C1C1=NNCCCCCCCC1 WADSJYLPJPTMLN-UHFFFAOYSA-N 0.000 description 4
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 4
- QCWXUUIWCKQGHC-UHFFFAOYSA-N Zirconium Chemical compound [Zr] QCWXUUIWCKQGHC-UHFFFAOYSA-N 0.000 description 4
- 150000004703 alkoxides Chemical class 0.000 description 4
- 238000010586 diagram Methods 0.000 description 4
- 229910052751 metal Inorganic materials 0.000 description 4
- 239000002184 metal Substances 0.000 description 4
- 239000000126 substance Substances 0.000 description 4
- WGTYBPLFGIVFAS-UHFFFAOYSA-M tetramethylammonium hydroxide Chemical compound [OH-].C[N+](C)(C)C WGTYBPLFGIVFAS-UHFFFAOYSA-M 0.000 description 4
- 229910052718 tin Inorganic materials 0.000 description 4
- 239000011135 tin Substances 0.000 description 4
- VXUYXOFXAQZZMF-UHFFFAOYSA-N titanium(IV) isopropoxide Chemical compound CC(C)O[Ti](OC(C)C)(OC(C)C)OC(C)C VXUYXOFXAQZZMF-UHFFFAOYSA-N 0.000 description 4
- 238000010438 heat treatment Methods 0.000 description 3
- 229910052742 iron Inorganic materials 0.000 description 3
- 229910052725 zinc Inorganic materials 0.000 description 3
- 239000011701 zinc Substances 0.000 description 3
- BMVXCPBXGZKUPN-UHFFFAOYSA-N 1-hexanamine Chemical compound CCCCCCN BMVXCPBXGZKUPN-UHFFFAOYSA-N 0.000 description 2
- UHOPWFKONJYLCF-UHFFFAOYSA-N 2-(2-sulfanylethyl)isoindole-1,3-dione Chemical compound C1=CC=C2C(=O)N(CCS)C(=O)C2=C1 UHOPWFKONJYLCF-UHFFFAOYSA-N 0.000 description 2
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 description 2
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 description 2
- 229910052782 aluminium Inorganic materials 0.000 description 2
- SMZOGRDCAXLAAR-UHFFFAOYSA-N aluminium isopropoxide Chemical compound [Al+3].CC(C)[O-].CC(C)[O-].CC(C)[O-] SMZOGRDCAXLAAR-UHFFFAOYSA-N 0.000 description 2
- ILRRQNADMUWWFW-UHFFFAOYSA-K aluminium phosphate Chemical compound O1[Al]2OP1(=O)O2 ILRRQNADMUWWFW-UHFFFAOYSA-K 0.000 description 2
- 229910000147 aluminium phosphate Inorganic materials 0.000 description 2
- 229940001007 aluminium phosphate Drugs 0.000 description 2
- NDKBVBUGCNGSJJ-UHFFFAOYSA-M benzyltrimethylammonium hydroxide Chemical compound [OH-].C[N+](C)(C)CC1=CC=CC=C1 NDKBVBUGCNGSJJ-UHFFFAOYSA-M 0.000 description 2
- YHWCPXVTRSHPNY-UHFFFAOYSA-N butan-1-olate;titanium(4+) Chemical compound [Ti+4].CCCC[O-].CCCC[O-].CCCC[O-].CCCC[O-] YHWCPXVTRSHPNY-UHFFFAOYSA-N 0.000 description 2
- 229910017052 cobalt Inorganic materials 0.000 description 2
- 239000010941 cobalt Substances 0.000 description 2
- 238000009833 condensation Methods 0.000 description 2
- 230000005494 condensation Effects 0.000 description 2
- 230000007812 deficiency Effects 0.000 description 2
- QGBSISYHAICWAH-UHFFFAOYSA-N dicyandiamide Chemical compound NC(N)=NC#N QGBSISYHAICWAH-UHFFFAOYSA-N 0.000 description 2
- XYIBRDXRRQCHLP-UHFFFAOYSA-N ethyl acetoacetate Chemical compound CCOC(=O)CC(C)=O XYIBRDXRRQCHLP-UHFFFAOYSA-N 0.000 description 2
- 229940093858 ethyl acetoacetate Drugs 0.000 description 2
- 238000001914 filtration Methods 0.000 description 2
- WWZKQHOCKIZLMA-UHFFFAOYSA-N octanoic acid Chemical compound CCCCCCCC(O)=O WWZKQHOCKIZLMA-UHFFFAOYSA-N 0.000 description 2
- 229910052710 silicon Inorganic materials 0.000 description 2
- 239000010703 silicon Substances 0.000 description 2
- IMFACGCPASFAPR-UHFFFAOYSA-N tributylamine Chemical compound CCCCN(CCCC)CCCC IMFACGCPASFAPR-UHFFFAOYSA-N 0.000 description 2
- 238000005303 weighing Methods 0.000 description 2
- 229940098697 zinc laurate Drugs 0.000 description 2
- XOOUIPVCVHRTMJ-UHFFFAOYSA-L zinc stearate Chemical compound [Zn+2].CCCCCCCCCCCCCCCCCC([O-])=O.CCCCCCCCCCCCCCCCCC([O-])=O XOOUIPVCVHRTMJ-UHFFFAOYSA-L 0.000 description 2
- 229940057977 zinc stearate Drugs 0.000 description 2
- LYSLZRDZOBAUFL-UHFFFAOYSA-L zinc;4-tert-butylbenzoate Chemical compound [Zn+2].CC(C)(C)C1=CC=C(C([O-])=O)C=C1.CC(C)(C)C1=CC=C(C([O-])=O)C=C1 LYSLZRDZOBAUFL-UHFFFAOYSA-L 0.000 description 2
- GPYYEEJOMCKTPR-UHFFFAOYSA-L zinc;dodecanoate Chemical compound [Zn+2].CCCCCCCCCCCC([O-])=O.CCCCCCCCCCCC([O-])=O GPYYEEJOMCKTPR-UHFFFAOYSA-L 0.000 description 2
- CHJMFFKHPHCQIJ-UHFFFAOYSA-L zinc;octanoate Chemical compound [Zn+2].CCCCCCCC([O-])=O.CCCCCCCC([O-])=O CHJMFFKHPHCQIJ-UHFFFAOYSA-L 0.000 description 2
- RYSXWUYLAWPLES-MTOQALJVSA-N (Z)-4-hydroxypent-3-en-2-one titanium Chemical compound [Ti].C\C(O)=C\C(C)=O.C\C(O)=C\C(C)=O.C\C(O)=C\C(C)=O.C\C(O)=C\C(C)=O RYSXWUYLAWPLES-MTOQALJVSA-N 0.000 description 1
- 229910052684 Cerium Inorganic materials 0.000 description 1
- 229910052691 Erbium Inorganic materials 0.000 description 1
- 229910052779 Neodymium Inorganic materials 0.000 description 1
- 229910052772 Samarium Inorganic materials 0.000 description 1
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical group [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 1
- 229910002808 Si–O–Si Inorganic materials 0.000 description 1
- UKLDJPRMSDWDSL-UHFFFAOYSA-L [dibutyl(dodecanoyloxy)stannyl] dodecanoate Chemical compound CCCCCCCCCCCC(=O)O[Sn](CCCC)(CCCC)OC(=O)CCCCCCCCCCC UKLDJPRMSDWDSL-UHFFFAOYSA-L 0.000 description 1
- 125000005595 acetylacetonate group Chemical group 0.000 description 1
- 239000004411 aluminium Substances 0.000 description 1
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 1
- KEBBHXFLBGHGMA-UHFFFAOYSA-K aluminum;4-ethyl-3-oxohexanoate Chemical compound [Al+3].CCC(CC)C(=O)CC([O-])=O.CCC(CC)C(=O)CC([O-])=O.CCC(CC)C(=O)CC([O-])=O KEBBHXFLBGHGMA-UHFFFAOYSA-K 0.000 description 1
- 150000001412 amines Chemical class 0.000 description 1
- 229910052787 antimony Inorganic materials 0.000 description 1
- 229910052788 barium Inorganic materials 0.000 description 1
- 229910052796 boron Inorganic materials 0.000 description 1
- 229910052791 calcium Inorganic materials 0.000 description 1
- 239000011575 calcium Substances 0.000 description 1
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 description 1
- 239000003086 colorant Substances 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000013005 condensation curing Methods 0.000 description 1
- 229920001577 copolymer Polymers 0.000 description 1
- 230000003247 decreasing effect Effects 0.000 description 1
- JQZRVMZHTADUSY-UHFFFAOYSA-L di(octanoyloxy)tin Chemical compound [Sn+2].CCCCCCCC([O-])=O.CCCCCCCC([O-])=O JQZRVMZHTADUSY-UHFFFAOYSA-L 0.000 description 1
- 125000004386 diacrylate group Chemical group 0.000 description 1
- AYOHIQLKSOJJQH-UHFFFAOYSA-N dibutyltin Chemical compound CCCC[Sn]CCCC AYOHIQLKSOJJQH-UHFFFAOYSA-N 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000007888 film coating Substances 0.000 description 1
- 238000009501 film coating Methods 0.000 description 1
- 229910052733 gallium Inorganic materials 0.000 description 1
- 229910052732 germanium Inorganic materials 0.000 description 1
- 229910052735 hafnium Inorganic materials 0.000 description 1
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 1
- 230000008676 import Effects 0.000 description 1
- 229910052738 indium Inorganic materials 0.000 description 1
- 229910052746 lanthanum Inorganic materials 0.000 description 1
- 239000011133 lead Substances 0.000 description 1
- 229910052749 magnesium Inorganic materials 0.000 description 1
- 239000011777 magnesium Substances 0.000 description 1
- 150000002739 metals Chemical class 0.000 description 1
- QJGQUHMNIGDVPM-UHFFFAOYSA-N nitrogen group Chemical group [N] QJGQUHMNIGDVPM-UHFFFAOYSA-N 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 238000004806 packaging method and process Methods 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- HKJYVRJHDIPMQB-UHFFFAOYSA-N propan-1-olate;titanium(4+) Chemical compound CCCO[Ti](OCCC)(OCCC)OCCC HKJYVRJHDIPMQB-UHFFFAOYSA-N 0.000 description 1
- XPGAWFIWCWKDDL-UHFFFAOYSA-N propan-1-olate;zirconium(4+) Chemical compound [Zr+4].CCC[O-].CCC[O-].CCC[O-].CCC[O-] XPGAWFIWCWKDDL-UHFFFAOYSA-N 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 125000005372 silanol group Chemical group 0.000 description 1
- 239000002002 slurry Substances 0.000 description 1
- 238000002791 soaking Methods 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
- 229910052712 strontium Inorganic materials 0.000 description 1
- 229910052715 tantalum Inorganic materials 0.000 description 1
- DAOVYDBYKGXFOB-UHFFFAOYSA-N tris(2-methylpropoxy)alumane Chemical compound [Al+3].CC(C)C[O-].CC(C)C[O-].CC(C)C[O-] DAOVYDBYKGXFOB-UHFFFAOYSA-N 0.000 description 1
- 229910052720 vanadium Inorganic materials 0.000 description 1
- 229910052727 yttrium Inorganic materials 0.000 description 1
- JDLYKQWJXAQNNS-UHFFFAOYSA-L zinc;dibenzoate Chemical compound [Zn+2].[O-]C(=O)C1=CC=CC=C1.[O-]C(=O)C1=CC=CC=C1 JDLYKQWJXAQNNS-UHFFFAOYSA-L 0.000 description 1
- 150000003755 zirconium compounds Chemical class 0.000 description 1
Images
Classifications
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L33/00—Semiconductor devices having potential barriers specially adapted for light emission; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof
- H01L33/48—Semiconductor devices having potential barriers specially adapted for light emission; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof characterised by the semiconductor body packages
- H01L33/50—Wavelength conversion elements
- H01L33/501—Wavelength conversion elements characterised by the materials, e.g. binder
- H01L33/502—Wavelength conversion materials
- H01L33/504—Elements with two or more wavelength conversion materials
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L33/00—Semiconductor devices having potential barriers specially adapted for light emission; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof
- H01L33/005—Processes
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L33/00—Semiconductor devices having potential barriers specially adapted for light emission; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof
- H01L33/48—Semiconductor devices having potential barriers specially adapted for light emission; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof characterised by the semiconductor body packages
- H01L33/50—Wavelength conversion elements
- H01L33/501—Wavelength conversion elements characterised by the materials, e.g. binder
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L25/00—Assemblies consisting of a plurality of individual semiconductor or other solid state devices ; Multistep manufacturing processes thereof
- H01L25/03—Assemblies consisting of a plurality of individual semiconductor or other solid state devices ; Multistep manufacturing processes thereof all the devices being of a type provided for in the same subgroup of groups H01L27/00 - H01L33/00, or in a single subclass of H10K, H10N, e.g. assemblies of rectifier diodes
- H01L25/04—Assemblies consisting of a plurality of individual semiconductor or other solid state devices ; Multistep manufacturing processes thereof all the devices being of a type provided for in the same subgroup of groups H01L27/00 - H01L33/00, or in a single subclass of H10K, H10N, e.g. assemblies of rectifier diodes the devices not having separate containers
- H01L25/075—Assemblies consisting of a plurality of individual semiconductor or other solid state devices ; Multistep manufacturing processes thereof all the devices being of a type provided for in the same subgroup of groups H01L27/00 - H01L33/00, or in a single subclass of H10K, H10N, e.g. assemblies of rectifier diodes the devices not having separate containers the devices being of a type provided for in group H01L33/00
- H01L25/0753—Assemblies consisting of a plurality of individual semiconductor or other solid state devices ; Multistep manufacturing processes thereof all the devices being of a type provided for in the same subgroup of groups H01L27/00 - H01L33/00, or in a single subclass of H10K, H10N, e.g. assemblies of rectifier diodes the devices not having separate containers the devices being of a type provided for in group H01L33/00 the devices being arranged next to each other
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L33/00—Semiconductor devices having potential barriers specially adapted for light emission; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof
- H01L33/44—Semiconductor devices having potential barriers specially adapted for light emission; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof characterised by the coatings, e.g. passivation layer or anti-reflective coating
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L2933/00—Details relating to devices covered by the group H01L33/00 but not provided for in its subgroups
- H01L2933/0008—Processes
- H01L2933/0033—Processes relating to semiconductor body packages
- H01L2933/0041—Processes relating to semiconductor body packages relating to wavelength conversion elements
Definitions
- the present invention relates to a method for producing dual color light emitting diodes (LEDs) and/or multi-color LEDs by one step film lamination.
- US 2013/221835 A1 which relates to a patterned lamination sheet incorporating an array of multiple light emitting devices, the sheet being formed by overlaying of components and one or more lamination steps
- US 2018/057714 A1 which relates to curable silicone compositions which may contain a phosphor, and are suitable for sheet-forming for use in optical devices such as packaging of semiconductor chips to form an LED
- US 2016/230084 A1 which describes a condensation curable silicone composition containing particulates such as phosphors and including a nitrogen-containing base.
- Dual color LEDs are now more and more popular in smart phones like iPhones as Flash and outdoor lighting.
- Flash there are generally two LEDs with different color (e.g., amber and white).
- the camera can adjust color of the flash to match what been determined to be the white balance of ambient light.
- Flash LED is an import application of colored phosphor films.
- Outdoor LED strip lamps with dual or more colors are also more and more popular in the market.
- current methods for producing dual color LEDs generally comprise two steps: (1) making two different color LEDs separately, and (2) then assembling two different color LEDs together (see, Fig. 1 , referred as old method 1).
- Another current method for producing dual color LED also comprises two steps: (1) adding a baffle between two LEDs, and (2) then dispensing two different silicone solutions with phosphor (see, Fig. 1 , referred as old method 2).
- old method 2 Another current method for producing dual color LEDs.
- above two old methods are suffered with some deficiencies, such as low production efficiency (which requires two steps), low color quality (since phosphor particles tends to be settled in silicone solutions).
- An objective of an exemplary embodiment of the present invention is to overcome the above and/or other deficiencies in the prior art.
- the inventors unexpectedly find that by controlling rheology performance (e.g., maximum tan ⁇ , minimum G' and curing time) of the colored phosphor compositions, two or more LEDs can be laminated with two or more colored phosphor films by one step film lamination, such that it may produce high color quality dual or multiple color LEDs with high production efficiency.
- two or more colored phosphor compositions may have close rheology performance (e.g., maximum tan ⁇ and gelling time).
- the present invention provides a method for producing dual-color LEDs or multi-color LEDs as defined in claim 1, comprising: laminating two or more LEDs with two or more colored phosphor films by one step film lamination; wherein each of the colored phosphor film comprises each other different colored phosphor composition which has a Maximum tan ⁇ ; and the difference of each Maximum tan ⁇ varies within a range of 0-30%.
- each of the different colored phosphor composition has a gelling time, and the difference of each gelling time varies within a range of 0-50%.
- the difference of each Maximum tan ⁇ varies within a range of 0-15%.
- the colored phosphor composition comprises a cure catalyst, a silicone binder and a phosphor; and the difference of gelling time and Maximum tan ⁇ is controlled by adjusting a ratio of the catalyst and silicone binder, and/or a ratio of the silicone binder and phosphor.
- the phosphor is pre-treated with a treatment agent, particularly when red or green phosphor is involved in phosphor film.
- the treatment agent is identical to the cure catalyst as used.
- the pre-treatment method comprises: (1) contacting the phosphor with treatment agent for a period time so as to ensure a good dispersion of phosphor in the treatment agent; and (2) drying the phosphor coated with the treatment agent, which is ready to be used with the silicone binder.
- the colored phosphor composition comprises a hydrosilylation curable organosiloxane composition and a phosphor.
- two or more LEDs are laminated with two or more colored phosphor films by one step film lamination.
- two or more colored phosphor compositions may have close rheology performance (e.g., maximum tan ⁇ and gelling time) by adjusting a ratio of a cure catalyst and silicone binder , and/or a ratio of the silicone binder and phosphor.
- two or more colored phosphor compositions may have close rheology performance (e.g., maximum tan ⁇ and gelling time) by using a hydrosilylation curable organosiloxane composition.
- the method for producing LED comprises: laminating two or more LEDs with two or more colored phosphor films by one step film lamination; wherein each of the colored phosphor film comprises each respectively a different colored phosphor composition which has a Maximum tan ⁇ ; the difference of each Maximum tan ⁇ varies within a range of 0-30%.
- the difference of each Maximum tan ⁇ varies within a range of 0-30%, 0-20%, 0-15%, 0-10%, 10-30%, 10-20%, 10-15%, 15-30%, 15-20%, or 20-30%.
- each Maximum tan ⁇ the difference of each Maximum tan ⁇
- the difference of each Maximum tan ⁇ larger Maximum tan ⁇ ⁇ smaller Maximum tan ⁇ smaller Maximum tan ⁇ ⁇ 100 %
- each of the colored phosphor films comprises each respectively different colored phosphor composition which may have a gelling time; the difference of each gelling time varies within a range of 0-50%.
- the difference of each gelling time varies within a range of 0-50%, 0-40%, 0-35%, 0-30%, 0-20%, 0-10%, 10-50%, 10-40%, 10-35%, 10-30%, 10-20%, 20-50%, 20-40%, 20-35%, 20-30%, 30-50%, 30-40%, 30-35%, 35-50%, 35-40%, or 40-50%.
- Figure 2 shows rheology profile of the uncured silicone binder system.
- said rheology profile is measured by rotational rheometer with the following conditions: (1) 25-150°C by 25 °C/min.; (2) 150°C for 30 min.; and (3) 0.1% distortion, 1.0Hz frequency, and by using 8 mm steel plate.
- the difference of each gelling time varies within a range of 0-50%, 0-40%, 0-35%, 0-30%, 0-20%, 0-10%, 10-50%, 10-40%, 10-35%, 10-30%, 10-20%, 20-50%, 20-40%, 20-35%, 20-30%, 30-50%, 30-40%, 30-35%, 35-50%, 35-40%, or 40-50%; and/or the difference of each Maximum tan ⁇ varies within a range of 0-30%, 0-20%, 0-15%, 0-10%, 10-30%, 10-20%, 10-15%, 15-30%, 15-20%, or 20-30%.
- the present inventors unexpected find that the difference of gelling time and Maximum tan ⁇ may be controlled by adjusting a ratio of the catalyst and silicone binder, and/or a ratio of the silicone binder and phosphor, so as to provide close rheology performance.
- the colored phosphor composition comprises a cure catalyst, a silicone binder and a phosphor; and the difference of gelling time and Maximum tan ⁇ is controlled by adjusting a ratio of the catalyst and silicone binder, and/or a ratio of the silicone binder and phosphor.
- phosphors are add together with a silicone bonder and catalyst, and solvent such as toluene is add to adjust viscosity of the composition to around 2000-8000 mPa ⁇ s for easy film coating.
- the slurry phosphor composition is coated on PET release liner by auto applicator.
- the wet phosphor film are then dry at room temperature for 5 min and then put in oven at a temperature of about 70°C for 30 min.
- the dried phosphor films are generally around 50-150 ⁇ m.
- the cure catalyst may be selected from any catalyst known in the art to effect condensation cure of organosiloxanes, such as various tin or titanium catalysts.
- Examples include, but are not limited to basic compounds, such as trimethylbenzylammonium hydroxide, tetramethylammonium hydroxide, n-hexylamine, tributylamine, diazabicycloundecene (DBU) and dicyandiamide; and metal-containing compounds such as tetraisopropyl titanate, tetrabutyl titanate, titanium acetylacetonate, aluminum triisobutoxide, aluminum triisopropoxide, zirconium tetra(acetylacetonato), zirconium tetrabutylate, cobalt octylate, cobalt acetylacetonato, iron acetylacetonato, tin acetylacetonato, dibutyltin octylate, dibutyltin laurate, zinc octylate, zinc bezoate, zinc p-tert-butyl
- the curing catalysts include zinc octylate, zinc benzoate, zinc p-tert- butylbenzoate, zinc laurate, zinc stearate, aluminium phosphate, and aluminum triisopropoxide. See, e.g. , U.S. Patent No. 8,193,269 .
- curing catalysts include, but are not limited to aluminum alkoxides, antimony alkoxides, barium alkoxides, boron alkoxides, calcium alkoxides, cerium alkoxides, erbium alkoxides, gallium alkoxides, silicon alkoxides, germanium alkoxides, hafnium alkoxides, indium alkoxides, iron alkoxides, lanthanum alkoxides, magnesium alkoxides, neodymium alkoxides, samarium alkoxides, strontium alkoxides, tantalum alkoxides, titanium alkoxides, tin alkoxides, vanadium alkoxide oxides, yttrium alkoxides, zinc alkoxides, zirconium alkoxides, titanium or zirconium compounds, especially titanium and zirconium alkoxides, and chel
- Double metal alkoxides are alkoxides containing two different metals in a particular ratio.
- the curing catalysts include titanium tetraethylate, titanium tetrapropylate, titanium tetraisopropylate, titanium tetrabutylate, titanium tetraisooctylate, titanium isopropylate tristearoylate, titanium truisopropylate stearoylate, titanium diisopropylate distearoylate, zirconium tetrapropylate, zirconium tetraisopropylate, zirconium tetrabutylate. See, e.g., U.S. Patent No. 7,005,460 .
- the curing catalysts include titanates, zirconates and hafnates as described in DE 4427528 C2 and EP 0 639 622 B1 .
- the curing catalyst comprises Dow Corning ® LF-9000 Film Encapsulant Catalyst (commercially available from DOW CORNING CORPORATION).
- treatment agent is used when handling specific phosphors like red one and etc.
- Treatment agent is similar with catalyst in effective composition while it is around 2-10 times higher concentration.
- the silicone binder may be selected from any silicone binder known in the art to form organosiloxane copolymer.
- the silicone binder may be solved in an organic solvent.
- the silicone binder may be those as described in WO 2013/134018 .
- the silicone binder comprises Dow Corning ® LF-1020 (commercially available from DOW CORNING CORPORATION).
- the phosphor may be selected from any phosphor known in the art. Examples thereof include, but are not limited to, YAG-04 phosphor (commercially available from Intematix Corporation), NYAG4454-L phosphor (commercially available from Intematix Corporation), BR-102L Phosphor (commercially available from Mitsubishi Chemical Corporation), GAL 550 Phosphor (commercially available from Intematix Corporation) or any combinations thereof.
- the phosphor may be pre-treated with a treatment agent, particularly when red or green phosphor is involved in phosphor film.
- the treatment agent is preferably a basic compounds, such as trimethylbenzylammonium hydroxide, tetramethylammonium hydroxide, n-hexylamine, tributylamine, diazabicycloundecene (DBU) and dicyandiamide.
- the pre-treatment method comprises: (1) contacting the phosphor with treatment agent for a period time so as to ensure a good dispersion of phosphor in the treatment agent; and (2) drying the phosphor coated with the treatment agent, which is ready to be used with the silicone binder.
- Phosphor pre-treatment is one way to lower down the impact of phosphor on silicone binder cure performance.
- the pre-treatment method comprises:
- the colored phosphor composition comprises a hydrosilylation curable organosiloxane composition and a phosphor.
- the hydrosilylation curable organosiloxane composition may comprise a hydrosilylation catalyst.
- the hydrosilylation curable organosiloxane composition comprises Dow Corning ® LF-1112 Phosphor Film Binder A&B Kit (commercially available from DOW CORNING CORPORATION).
- the hydrosilylation curable organosiloxane composition may be those as described in WO 2016/022332A1 .
- the method for producing a LED may greatly improve production efficiency (i.e., dual and multi-color LEDs in one step) and lower cost of ownership. Further, it may improve uniformity of phosphor dispersion, thereby improve color quality of LEDs.
- Ranges can be expressed herein as from “about” one particular value, and/or to “about” another particular value. When such a range is expressed, examples include from the one particular value and/or to the other particular value. Similarly, when values are expressed as approximations, by use of the antecedent "about,” it will be understood that the particular value forms another aspect. It will be further understood that the endpoints of each of the ranges are significant both in relation to the other endpoint, and independently of the other endpoint.
- the rheology performance is measured by TA ARES G2 rheometer using following conditions: (1) 15-150°C by 25 °C/min.; (2) 150°C for 30 min.; and (3) 0.5% strain, 1.0Hz frequency, and by using 8 mm steel plate.
- Silicone Binder 1 Catalyst 1 Gelling time (sec.) Max. tan ⁇ 100 : 1 1224 2.21 100 : 1.5 510 1.79 100 : 2 315 1.25
- the ratios of Silicone binder 1 to Catalyst 1 are 100: 2, 100:2.5 and 100: 3, respectively. And the ratio of Silicone binder 1 to Phosphor 2 is 100:100.
- the rheology performance is measured by TA ARES G2 rheometer using following conditions: (1) 15-150°C by 25 °C/min.; (2) 150°C for 30 min.; and (3) 0.5% strain, 1.0Hz frequency, and by using 8 mm steel plate.
- Silicone Binder 1 Catalyst 1 Gelling time (sec.) Max. tan ⁇ 100 : 2 515 1.84 100 : 2.5 356 1.49 100 : 3 309 1.34
- Example 1 One step film lamination
- the phosphor films as obtained in Reference Examples 1 and 2 are laminated by Fulin PLC-100A vacuum laminator.
- the lamination conditions are as follows:
- two different colored phosphor films are successfully laminated on LEDs in one step film lamination, which exhibits uniform phosphor dispersion and better color quality.
- Example 2 red phosphor pre-treatment and dual color phosphor film lamination.
- the ratio of Silicone binder 1 to Catalyst 1 is 100:1.5.
- the ratio of Silicone binder 1 to Phosphors 1 and 3 is 100:56.
- the ratio of Phosphor 1 to Phosphor 3 is 40:1.
- BR-102L is pretreated with treatment agent following below procedure:
- the rheology performance is measured by TA ARES G2 rheometer using following conditions: (1) 15-150°C by 25 °C/min.; (2) 150°C for 20 min.; and (3) 0.5% strain, 1.0Hz frequency, and by using 8 mm steel plate.
- the ratio of Silicone binder 1 to Catalyst 1 is 100:1.
- the ratio of Silicone bonder 1 to Phosphors 1 and 3 is 100:139.
- the ratio of Phosphor 1 to Phosphor 3 is 2:1.
- BR-102L is pretreated with treatment agent following above similar procedure.
- the rheology performance is measured by TA ARES G2 rheometer using following conditions: (1) 15-150°C by 25 °C/min.; (2) 150°C for 20min.; and (3) 0.5% strain, 1.0Hz frequency, and by using 8 mm steel plate.
- Example 3 hydrosilylation cure dual color phosphor film preparation and lamination.
- the rheology performance is measured by TA ARES G2 rheometer using following conditions: (1) 15-125°C by 20 °C/min.; (2) 125°C for 30min.; and (3) 0.5% strain, 1.0Hz frequency, and by using 8 mm steel plate.
- the ratio of Silicone binder 4 to Phosphors 1 and 5 is 100:110.
- the ratio of Phosphor 1 to Phosphor 5 is 10:1.
- the rheology performance is measured by TA ARES G2 rheometer using following conditions: (1) 15-125°C by 20 °C/min.; (2) 125°C for 30min.; and (3) 0.5% strain, 1.0Hz frequency, and by using 8 mm steel plate.
- Example 3 in cased of a hydrosilylation curable composition, phosphor will not impact silicone binder system's Rheology performance, thereby curing performance. So it not necessary to adjust the mix ratio of silicone binder to phosphor.
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Description
- The present invention relates to a method for producing dual color light emitting diodes (LEDs) and/or multi-color LEDs by one step film lamination.
- The following documents may be useful in understanding the background to the present disclosure:
US 2013/221835 A1 which relates to a patterned lamination sheet incorporating an array of multiple light emitting devices, the sheet being formed by overlaying of components and one or more lamination steps;US 2018/057714 A1 which relates to curable silicone compositions which may contain a phosphor, and are suitable for sheet-forming for use in optical devices such as packaging of semiconductor chips to form an LED; andUS 2016/230084 A1 which describes a condensation curable silicone composition containing particulates such as phosphors and including a nitrogen-containing base. - Dual color LEDs (or multi-color LEDs) are now more and more popular in smart phones like iPhones as Flash and outdoor lighting. In terms of application in Flash, there are generally two LEDs with different color (e.g., amber and white). By adjusting their ratio, the camera can adjust color of the flash to match what been determined to be the white balance of ambient light. Flash LED is an import application of colored phosphor films. Outdoor LED strip lamps with dual or more colors are also more and more popular in the market.
- However, current methods for producing dual color LEDs generally comprise two steps: (1) making two different color LEDs separately, and (2) then assembling two different color LEDs together (see,
Fig. 1 , referred as old method 1). Another current method for producing dual color LED also comprises two steps: (1) adding a baffle between two LEDs, and (2) then dispensing two different silicone solutions with phosphor (see,Fig. 1 , referred as old method 2). Currently, above two old methods are suffered with some deficiencies, such as low production efficiency (which requires two steps), low color quality (since phosphor particles tends to be settled in silicone solutions). - Accordingly, there is a need to provide a novel method for producing dual color LEDs and multi-color LEDs, which can produce high color quality dual/multiple color LEDs with high production efficiency.
- An objective of an exemplary embodiment of the present invention is to overcome the above and/or other deficiencies in the prior art. The inventors unexpectedly find that by controlling rheology performance (e.g., maximum tan δ, minimum G' and curing time) of the colored phosphor compositions, two or more LEDs can be laminated with two or more colored phosphor films by one step film lamination, such that it may produce high color quality dual or multiple color LEDs with high production efficiency.
- In the present invention, by adjusting a ratio of a cure catalyst and silicone binder, or using a hydrosilylation curable organosiloxane composition, two or more colored phosphor compositions may have close rheology performance (e.g., maximum tan δ and gelling time).
- Thus, the present invention provides a method for producing dual-color LEDs or multi-color LEDs as defined in
claim 1, comprising: laminating two or more LEDs with two or more colored phosphor films by one step film lamination; wherein each of the colored phosphor film comprises each other different colored phosphor composition which has a Maximum tan δ; and the difference of each Maximum tan δ varies within a range of 0-30%. - In one embodiment of the present invention, each of the different colored phosphor composition has a gelling time, and the difference of each gelling time varies within a range of 0-50%.
- In one embodiment of the present invention, the difference of each Maximum tan δ varies within a range of 0-15%.
- In one embodiment of the present invention, the colored phosphor composition comprises a cure catalyst, a silicone binder and a phosphor; and the difference of gelling time and Maximum tan δ is controlled by adjusting a ratio of the catalyst and silicone binder, and/or a ratio of the silicone binder and phosphor.
- In one embodiment of the present invention, the phosphor is pre-treated with a treatment agent, particularly when red or green phosphor is involved in phosphor film. In some embodiments, the treatment agent is identical to the cure catalyst as used. The pre-treatment method comprises: (1) contacting the phosphor with treatment agent for a period time so as to ensure a good dispersion of phosphor in the treatment agent; and (2) drying the phosphor coated with the treatment agent, which is ready to be used with the silicone binder.
- In one embodiment of the present invention, the colored phosphor composition comprises a hydrosilylation curable organosiloxane composition and a phosphor.
- Other features and aspects will become apparent from the following Detailed Description, the Drawings and the Claims.
- The present invention can be understood better in light of the description of exemplary embodiments of the present invention with reference to the accompanying drawings, in which:
-
FIG. 1 is a schematic diagram showing current methods for producing dual color LED (old methods 1 and 2) and an inventive method for producing dual color LEDs. -
FIG. 2 is a diagram showing rheology profile of uncured silicone binder system in the present invention. -
FIG. 3 is a schematic diagram showing an exemplary embodiment (Example 2) of the method for producing dual color LEDs in the present invention. -
FIG. 4 is a schematic diagram showing an exemplary embodiment (Example 3) of the method for producing dual color LEDs in the present invention. - Hereafter, a detailed description will be given for preferred embodiments of the present disclosure.
- In the present invention, the inventors find that by controlling rheology performance (e.g., maximum tan δ and gelling time) of the colored phosphor compositions, two or more LEDs are laminated with two or more colored phosphor films by one step film lamination. In one embodiment, two or more colored phosphor compositions may have close rheology performance (e.g., maximum tan δ and gelling time) by adjusting a ratio of a cure catalyst and silicone binder, and/or a ratio of the silicone binder and phosphor. In another embodiment, two or more colored phosphor compositions may have close rheology performance (e.g., maximum tan δ and gelling time) by using a hydrosilylation curable organosiloxane composition.
- In the present invention, the method for producing LED comprises: laminating two or more LEDs with two or more colored phosphor films by one step film lamination; wherein each of the colored phosphor film comprises each respectively a different colored phosphor composition which has a Maximum tan δ; the difference of each Maximum tan δ varies within a range of 0-30%.
- In one embodiment of the present invention, the difference of each Maximum tan δ varies within a range of 0-30%, 0-20%, 0-15%, 0-10%, 10-30%, 10-20%, 10-15%, 15-30%, 15-20%, or 20-30%.
-
- In one embodiment of the present invention, each of the colored phosphor films comprises each respectively different colored phosphor composition which may have a gelling time; the difference of each gelling time varies within a range of 0-50%.
- In one embodiment of the present invention, the difference of each gelling time varies within a range of 0-50%, 0-40%, 0-35%, 0-30%, 0-20%, 0-10%, 10-50%, 10-40%, 10-35%, 10-30%, 10-20%, 20-50%, 20-40%, 20-35%, 20-30%, 30-50%, 30-40%, 30-35%, 35-50%, 35-40%, or 40-50%.
-
- The term, "Maximum tan δ (or Max. tan δ)", as used herein, refers to maximum tan δ = loss modulus/storage modulus, which is used to characterize the silicone binder system's flowability capability at heating temperature. The term, "gelling time", as used herein is defined by time from Max. tan δ to tan δ=1, which is used to characterize how fast the silicone binder system cures. Said gelling time and Max. tan δ are most two important rheology performances for success phosphor one-step film lamination.
- In general, uncured silicone binder system will flow first with temperature increase and then get cured.
Figure 2 shows rheology profile of the uncured silicone binder system. In the present invention, said rheology profile is measured by rotational rheometer with the following conditions: (1) 25-150°C by 25 °C/min.; (2) 150°C for 30 min.; and (3) 0.1% distortion, 1.0Hz frequency, and by using 8 mm steel plate. - Since the curing performance of silicone binder system would be affected by various phosphor. For one step film lamination, two or more different colored phosphor composition should be tuned to provide close rheology performance (e.g., gelling time and maximum tan δ). In one embodiment of the present invention, the difference of each gelling time varies within a range of 0-50%, 0-40%, 0-35%, 0-30%, 0-20%, 0-10%, 10-50%, 10-40%, 10-35%, 10-30%, 10-20%, 20-50%, 20-40%, 20-35%, 20-30%, 30-50%, 30-40%, 30-35%, 35-50%, 35-40%, or 40-50%; and/or the difference of each Maximum tan δ varies within a range of 0-30%, 0-20%, 0-15%, 0-10%, 10-30%, 10-20%, 10-15%, 15-30%, 15-20%, or 20-30%. On the other hand, the more catalyst, the colored phosphor composition would cure fast. Thus, the present inventors unexpected find that the difference of gelling time and Maximum tan δ may be controlled by adjusting a ratio of the catalyst and silicone binder, and/or a ratio of the silicone binder and phosphor, so as to provide close rheology performance.
- In one embodiment of the present invention, the colored phosphor composition comprises a cure catalyst, a silicone binder and a phosphor; and the difference of gelling time and Maximum tan δ is controlled by adjusting a ratio of the catalyst and silicone binder, and/or a ratio of the silicone binder and phosphor. In most embodiments, phosphors are add together with a silicone bonder and catalyst, and solvent such as toluene is add to adjust viscosity of the composition to around 2000-8000 mPa·s for easy film coating. After mixing, the slurry phosphor composition is coated on PET release liner by auto applicator. The wet phosphor film are then dry at room temperature for 5 min and then put in oven at a temperature of about 70°C for 30 min. The dried phosphor films are generally around 50-150 µm.
- In the present invention, the cure catalyst may be selected from any catalyst known in the art to effect condensation cure of organosiloxanes, such as various tin or titanium catalysts. Curing catalyst can be any curing catalyst that may be used to promote condensation of silicon bonded hydroxy (=silanol) groups to form Si-O-Si linkages. Examples include, but are not limited to, amines and complexes of lead, tin, titanium, zinc, and iron. Other examples include, but are not limited to basic compounds, such as trimethylbenzylammonium hydroxide, tetramethylammonium hydroxide, n-hexylamine, tributylamine, diazabicycloundecene (DBU) and dicyandiamide; and metal-containing compounds such as tetraisopropyl titanate, tetrabutyl titanate, titanium acetylacetonate, aluminum triisobutoxide, aluminum triisopropoxide, zirconium tetra(acetylacetonato), zirconium tetrabutylate, cobalt octylate, cobalt acetylacetonato, iron acetylacetonato, tin acetylacetonato, dibutyltin octylate, dibutyltin laurate, zinc octylate, zinc bezoate, zinc p-tert-butylbenzoate, zinc laurate, zinc stearate, aluminium phosphate, and alminium triisopropoxide; organic titanium chelates such as aluminium trisacetylacetonate, aluminium bisethylacetoacetate monoacetylacetonate, diisopropoxybis(ethylacetoacetate)titanium, and diisopropoxybis(ethylacetoacetate)titanium. In some embodiments, the curing catalysts include zinc octylate, zinc benzoate, zinc p-tert- butylbenzoate, zinc laurate, zinc stearate, aluminium phosphate, and aluminum triisopropoxide. See, e.g. ,
U.S. Patent No. 8,193,269 . Other examples of curing catalysts include, but are not limited to aluminum alkoxides, antimony alkoxides, barium alkoxides, boron alkoxides, calcium alkoxides, cerium alkoxides, erbium alkoxides, gallium alkoxides, silicon alkoxides, germanium alkoxides, hafnium alkoxides, indium alkoxides, iron alkoxides, lanthanum alkoxides, magnesium alkoxides, neodymium alkoxides, samarium alkoxides, strontium alkoxides, tantalum alkoxides, titanium alkoxides, tin alkoxides, vanadium alkoxide oxides, yttrium alkoxides, zinc alkoxides, zirconium alkoxides, titanium or zirconium compounds, especially titanium and zirconium alkoxides, and chelates and oligo- and polycondensates of the above alkoxides, dialkyltin diacetate, tin(II) octoate, dialkyltin diacrylate, dialkyltin oxide and double metal alkoxides. Double metal alkoxides are alkoxides containing two different metals in a particular ratio. In some embodiments, the curing catalysts include titanium tetraethylate, titanium tetrapropylate, titanium tetraisopropylate, titanium tetrabutylate, titanium tetraisooctylate, titanium isopropylate tristearoylate, titanium truisopropylate stearoylate, titanium diisopropylate distearoylate, zirconium tetrapropylate, zirconium tetraisopropylate, zirconium tetrabutylate. See, e.g.,U.S. Patent No. 7,005,460 . In addition, the curing catalysts include titanates, zirconates and hafnates as described inDE 4427528 C2 andEP 0 639 622 B1 - In the present invention, treatment agent is used when handling specific phosphors like red one and etc. Treatment agent is similar with catalyst in effective composition while it is around 2-10 times higher concentration.
- In the present invention, the silicone binder may be selected from any silicone binder known in the art to form organosiloxane copolymer. In some embodiments, the silicone binder may be solved in an organic solvent. Also, the silicone binder may be those as described in
WO 2013/134018 . In some embodiments, the silicone binder comprises Dow Corning® LF-1020 (commercially available from DOW CORNING CORPORATION). - In the present invention, the phosphor may be selected from any phosphor known in the art. Examples thereof include, but are not limited to, YAG-04 phosphor (commercially available from Intematix Corporation), NYAG4454-L phosphor (commercially available from Intematix Corporation), BR-102L Phosphor (commercially available from Mitsubishi Chemical Corporation), GAL 550 Phosphor (commercially available from Intematix Corporation) or any combinations thereof.
- In one embodiment of the present invention, the phosphor may be pre-treated with a treatment agent, particularly when red or green phosphor is involved in phosphor film. In some embodiments, the treatment agent is preferably a basic compounds, such as trimethylbenzylammonium hydroxide, tetramethylammonium hydroxide, n-hexylamine, tributylamine, diazabicycloundecene (DBU) and dicyandiamide. The pre-treatment method comprises: (1) contacting the phosphor with treatment agent for a period time so as to ensure a good dispersion of phosphor in the treatment agent; and (2) drying the phosphor coated with the treatment agent, which is ready to be used with the silicone binder. Phosphor pre-treatment is one way to lower down the impact of phosphor on silicone binder cure performance.
- For example, the pre-treatment method comprises:
- Weighing a phosphor and a treating agent in a ratio of 1:1;
- Charging the phosphor and a treating agent in a closed sealed container;
- mixing and soaking the phosphor in the treating agent for 4 hours, so as to ensure a good dispersion of phosphor in the treatment agent solution;
- Filtering out the phosphor or using other method to separate phosphor from the treating agent; and
- Putting the wet phosphor into a drying oven and heating up to 150°C for 8 hours, so as to provide dried phosphor which is ready to be used for formulations.
- In one embodiment of the present invention, the colored phosphor composition comprises a hydrosilylation curable organosiloxane composition and a phosphor. The hydrosilylation curable organosiloxane composition may comprise a hydrosilylation catalyst. In some embodiments, the hydrosilylation curable organosiloxane composition comprises Dow Corning® LF-1112 Phosphor Film Binder A&B Kit (commercially available from DOW CORNING CORPORATION). Also, the hydrosilylation curable organosiloxane composition may be those as described in
WO 2016/022332A1 . - In the present invention, the method for producing a LED may greatly improve production efficiency (i.e., dual and multi-color LEDs in one step) and lower cost of ownership. Further, it may improve uniformity of phosphor dispersion, thereby improve color quality of LEDs.
- Ranges can be expressed herein as from "about" one particular value, and/or to "about" another particular value. When such a range is expressed, examples include from the one particular value and/or to the other particular value. Similarly, when values are expressed as approximations, by use of the antecedent "about," it will be understood that the particular value forms another aspect. It will be further understood that the endpoints of each of the ranges are significant both in relation to the other endpoint, and independently of the other endpoint.
- Unless otherwise expressly stated, it is in no way intended that any method set forth herein be construed as requiring that its steps be performed in a specific order. Accordingly, where a method claim does not actually recite an order to be followed by its steps or it is not otherwise specifically stated in the claims or descriptions that the steps are to be limited to a specific order, it is no way intended that any particular order be inferred.
- The materials as used in Reference Example 1 are as follows:
- Silicone binder 1: Dow Corning® LF-1020 Phosphor Film Binder, 5g, commercially available from DOW CORNING CORPORATION;
- Catalyst 1: Dow Corning® LF-9000 Film Encapsulant Catalyst, 0.075g, commercially available from DOW CORNING CORPORATION; and
- Phosphor 1: YAG-04 phosphor, 5g, commercially available from Intematix Corporation.
- In Reference Example 1, the ratios of
Silicone binder 1 toCatalyst 1 are 100: 1, 100:1.5 and 100: 2, respectively. And the ratio ofSilicone binder 1 toPhosphor 1 is 100:100. - Sample preparation (taking a ratio of
Silicone binder 1 toCatalyst 1=100:1.5 as example) - (1) providing
5g Phosphor 1 with5g Silicone binder 1 and 0.075g Catalyst 1, with adding 0.3g toluene as organic solvent to adjust the viscosity, and mixing in a ThinkyARV-310 planetary vacuum mixer to provide a mixed slurry; - (2) using Hohsen auto applicator, coating the mixed slurry on a PET release liner;
- (3) drying the PET release liner at room temperature for 5 min. and then put it into a drying oven at a temperature of 70°C for 30 min., resulting in a dry film with a thickness of 75 µm.
- The rheology performance is measured by TA ARES G2 rheometer using following conditions: (1) 15-150°C by 25 °C/min.; (2) 150°C for 30 min.; and (3) 0.5% strain, 1.0Hz frequency, and by using 8 mm steel plate.
Silicone Binder 1 : Catalyst 1Gelling time (sec.) Max. tan δ 100 : 1 1224 2.21 100 : 1.5 510 1.79 100 : 2 315 1.25 - The materials as used in Reference Example 2 are as follows:
- Silicone binder 1: Dow Corning® LF-1020 Phosphor Film Binder, 5g, commercially available from DOW CORNING CORPORATION;
- Catalyst 1: Dow Corning® LF-9000 Film Encapsulant Catalyst, 0.1g, commercially available from DOW CORNING CORPORATION; and
- Phosphor 2: NYAG4454-L phosphor, 5g, commercially available from Intematix Corporation.
- In Reference Example 2, the ratios of
Silicone binder 1 toCatalyst 1 are 100: 2, 100:2.5 and 100: 3, respectively. And the ratio ofSilicone binder 1 toPhosphor 2 is 100:100. - Sample preparation (taking a ratio of
Silicone binder 1 toCatalyst 1=100:2 as example) - (1) providing
5g Phosphor 2 with5g Silicone binder 1 and 0.1g Catalyst 1, with adding 0.3g toluene as organic solvent to adjust the viscosity, and mixing in a ThinkyARV-310 planetary vacuum mixer to provide a mixed slurry; - (2) using Hohsen auto applicator, coating the mixed slurry on a PET release liner;
- (3) drying the PET release liner at room temperature for 5 min. and then put it into a drying oven at a temperature of 70°C for 30 min., resulting in a dry film with a thickness of 75 µm.
- The rheology performance is measured by TA ARES G2 rheometer using following conditions: (1) 15-150°C by 25 °C/min.; (2) 150°C for 30 min.; and (3) 0.5% strain, 1.0Hz frequency, and by using 8 mm steel plate.
Silicone Binder 1 : Catalyst 1Gelling time (sec.) Max. tan δ 100 : 2 515 1.84 100 : 2.5 356 1.49 100 : 3 309 1.34 - From above Reference Examples 1 and 2, it could be noted that for close rheology performance, the ratio of
Silicone binder 1 toCatalyst 1 for NYAG4454-L phosphor should be decreased to 100:2 in comparison with said "100:1.5" for YAG-04 phosphor. The difference of the gelling time varies within 1%; and the difference of each Maximum tan δ varies within 2.8%. - The phosphor films as obtained in Reference Examples 1 and 2 are laminated by Fulin PLC-100A vacuum laminator. The lamination conditions are as follows:
- Lamination temperature: 124.6°C ;
- Lamination time: 300 seconds; and
- Vacuum: 0.34 kPa
- In this example, two different colored phosphor films are successfully laminated on LEDs in one step film lamination, which exhibits uniform phosphor dispersion and better color quality.
- The materials as used are as follows:
- Silicone binder 1: Dow Corning® LF-1020 Phosphor Film Binder, 5g, commercially available from DOW CORNING CORPORATION;
- Catalyst 1: Dow Corning® LF-9000 Film Encapsulant Catalyst, 0.075g, commercially available from DOW CORNING CORPORATION; and
- Phosphor 1: YAG-04 Phosphor, commercially available from Intematix Corporation.
- Phosphor 3: BR-102L Phosphor, commercially available from Mitsubishi Chemical Corporation.
- In 3C formulation, the ratio of
Silicone binder 1 toCatalyst 1 is 100:1.5. And the ratio ofSilicone binder 1 toPhosphors 1 and 3 is 100:56. The ratio ofPhosphor 1 to Phosphor 3 is 40:1. BR-102L is pretreated with treatment agent following below procedure: - Weighing the phosphor 3 and the treating agent in a ratio of 1:1.
- Charging them in an appropriate container and closely tight it.
- Using mixer to soak the phosphor in the treating agent for 4 hours and ensure a good dispersion of phosphor in the solution.
- Filtering out the phosphor to separate phosphor from the treating agent.
- Putting the wet phosphor into a drying oven and heating up to 150°C for 8 hours.
- The dried phosphor is ready to be used for formulations.
-
- (1) providing 2.732
g Phosphor 1 and 0.068g Phosphor 3 with5g Silicone binder 1 and 0.075g Catalyst 1, with adding 0.3g toluene as organic solvent to adjust the viscosity, and mixing in a ThinkyARV-310 planetary vacuum mixer to provide a mixed slurry; - (2) using Hohsen auto applicator, coating the mixed slurry on a PET release liner;
- (3) drying the PET release liner at room temperature for 5 min. and then put it into a drying oven at a temperature of 70°C for 30 min., resulting in a dry film with a thickness of 80 µm.
- The rheology performance is measured by TA ARES G2 rheometer using following conditions: (1) 15-150°C by 25 °C/min.; (2) 150°C for 20 min.; and (3) 0.5% strain, 1.0Hz frequency, and by using 8 mm steel plate.
- The materials as used are as follows:
- Silicone binder 1: Dow Corning® LF-1020 Phosphor Film Binder, 5g, commercially available from DOW CORNING CORPORATION;
- Catalyst 1: Dow Corning® LF-9000 Film Encapsulant Catalyst, 0.050g, commercially available from DOW CORNING CORPORATION; and
- Phosphor 1: YAG-04 Phosphor, commercially available from Intematix Corporation.
- Phosphor 3: BR-102L Phosphor, commercially available from Mitsubishi Chemical Corporation.
- In 3W formulation, the ratio of
Silicone binder 1 toCatalyst 1 is 100:1. And the ratio ofSilicone bonder 1 toPhosphors 1 and 3 is 100:139. The ratio ofPhosphor 1 to Phosphor 3 is 2:1. BR-102L is pretreated with treatment agent following above similar procedure. -
- (1) providing 4.633
g Phosphor 1 and 2.317g Phosphor 3 with5g Silicone binder 1 and 0.050g Catalyst 1, with adding 0.5g toluene as organic solvent to adjust the viscosity, and mixing in a ThinkyARV-310 planetary vacuum mixer to provide a mixed slurry; - (2) using Hohsen auto applicator, coating the mixed slurry on a PET release liner;
- (3) drying the PET release liner at room temperature for 5 min. and then put it into a drying oven at a temperature of 70°C for 30 min., resulting in a dry film with a thickness of 86 µm.
- The rheology performance is measured by TA ARES G2 rheometer using following conditions: (1) 15-150°C by 25 °C/min.; (2) 150°C for 20min.; and (3) 0.5% strain, 1.0Hz frequency, and by using 8 mm steel plate.
- Cold white and warm white phosphor films' rheology performances are listed in below table.
Phosphor film Gelling time (sec.) Max. tan δ 3C 526 1.36 3W 360 1.48 - Cold white and warm white phosphor films 3C and 3W are laminated by Fulin PLC-100A vacuum laminator. Detailed lamination condition:
- Lamination temperature: 124.6°C;
- Lamination time: 300 seconds; and
- Vacuum: 0.34 kPa
- As shown in
Fig. 3 , Cold white and warm white phosphor films 3C and 3W are successfully laminated on LEDs in one step film lamination, which exhibits uniform phosphor dispersion and better color quality. - The materials as used are as follows:
- Silicone binder 4: Dow Corning® LF-1112 Phosphor Film Binder Part A + Part B (1:1), 5g, commercially available from DOW CORNING CORPORATION;
- Phosphor 1: YAG-04 Phosphor, commercially available from Intematix Corporation..
- Phosphor 4 : GAL550 Phosphor, commercially available from Intematix Corporation..
- In 4C formulation, the ratio of Silicone binder 4 to
Phosphors 1 and 4 is 100:27. The ratio ofPhosphor 1 to Phosphor 4 is 5:1. -
- (1) providing 1.125
g Phosphor 1 and 0.225g Phosphor 4 with 2.5g part A of Silicone binder 4 and 2.5g part B of Silicone binder 4, with adding 0.3g propyl propionate as organic solvent to adjust the viscosity, and mixing in a ThinkyARV-310 planetary vacuum mixer to provide a mixed slurry; - (2) using Hohsen auto applicator, coating the mixed slurry on a PET release liner;
- (3) drying the PET release liner at room temperature for 5 min. and then put it into a drying oven at a temperature of 70°C for 30 min., resulting in a dry film with a thickness of 52 µm.
- The rheology performance is measured by TA ARES G2 rheometer using following conditions: (1) 15-125°C by 20 °C/min.; (2) 125°C for 30min.; and (3) 0.5% strain, 1.0Hz frequency, and by using 8 mm steel plate.
- The materials as used are as follows:
- Silicone binder 4: Dow Corning® LF-1112 Phosphor Film Binder Part A + Part B (1:1), 5g, commercially available from DOW CORNING CORPORATION;
- Phosphor 1: YAG-04 Phosphor, commercially available from Intematix Corporation.
- Phosphor 5: MPR-1003 Phosphor, commercially available from Mitsubishi Chemical Corporation.
- In 4W formulation, the ratio of Silicone binder 4 to
Phosphors 1 and 5 is 100:110. The ratio ofPhosphor 1 to Phosphor 5 is 10:1. -
- (1) providing
5g Phosphor 1 and 0.5g Phosphor 5 with 2.5g part A of Silicone binder 4 and 2.5g part B of Silicone binder 4, with adding 0.5g propyl propionate as organic solvent to adjust the viscosity, and mixing in a ThinkyARV-310 planetary vacuum mixer to provide a mixed slurry; - (2) using Hohsen auto applicator, coating the mixed slurry on a PET release liner;
- (3) drying the PET release liner at room temperature for 5 min. and then put it into a drying oven at a temperature of 70°C for 30 min., resulting in a dry film with a thickness of 86 µm.
- The rheology performance is measured by TA ARES G2 rheometer using following conditions: (1) 15-125°C by 20 °C/min.; (2) 125°C for 30min.; and (3) 0.5% strain, 1.0Hz frequency, and by using 8 mm steel plate.
- Cold white and warm white phosphor films' rheology performances are listed in below table.
Phosphor film Gelling time (sec.) Max. tan δ 4C 386 1.70 4W 280 1.49 - As shown in Example 3, in cased of a hydrosilylation curable composition, phosphor will not impact silicone binder system's Rheology performance, thereby curing performance. So it not necessary to adjust the mix ratio of silicone binder to phosphor.
- Cold white and warm white phosphor films 4C and 4W are laminated by Fulin PLC-100A vacuum laminator. The lamination conditions are as follows:
- Lamination temperature: 121.8°C;
- Lamination time: 300 seconds; and
- Vacuum: 0.34 kPa
- As shown in
Fig. 4 , Cold white and warm white phosphor films 4C and 4W are successfully laminated on LEDs in one step film lamination, which exhibits uniform phosphor dispersion and better color quality. - The above descriptions are merely embodiments of the invention and are not intended to restrict the scope of the invention, which is defined by the scope of the appended claims.
Claims (8)
- A method for producing dual-color LEDs and/or multi-color LEDs by lamination of LEDs with colored phosphor film, comprising:laminating two or more LEDs with two or more colored phosphor films by one step film lamination thereby producing dual and/or multi-color LEDs from two or more LEDs and two or more colored phosphor films in one step;wherein each of the colored phosphor films comprises each respectively a different colored phosphor composition which has a Maximum tan δ; andthe difference of each Maximum tan δ varies within a range of 0-30%,each colored phosphor composition comprising a silicone binder.
- The method according to claim 1, wherein each of the different colored phosphor composition has a gelling time, and the difference of each gelling time varies within a range of 0-50%.
- The method according to claim 1, wherein the difference of each Maximum tan δ varies within a range of 0-15%.
- The method according to claim 1, wherein the colored phosphor composition comprises a cure catalyst, and a phosphor; and
the difference of Maximum tan δ is controlled by adjusting a ratio of the catalyst and silicone binder, and/or a ratio of the silicone binder and phosphor. - The method according to claim 2, wherein the colored phosphor composition comprises a cure catalyst, and a phosphor; and
the difference of gelling time and/or Maximum tan δ is controlled by adjusting a ratio of the catalyst and silicone binder, and/or a ratio of the silicone binder and phosphor. - The method according to claim 4 or 5, wherein the phosphor is pre-treated with a treatment agent.
- The method according to claim 6, wherein the treatment agent is a basic compound.
- The method according to claim 6, wherein the phosphor is pre-treated by the following method: (1) contacting the phosphor with treatment agent for a period time so as to ensure a good dispersion of phosphor in the treatment agent; and (2) drying the phosphor coated with the treatment agent, which is ready to be used with the silicone binder.
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PCT/CN2018/087460 WO2019218336A1 (en) | 2018-05-18 | 2018-05-18 | Method for producing led by one step film lamination |
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